Spinning artificial materials



Patented June .27, 1950 UNITED STATES, PATENT OFFICE SPINNING ARTIFICIAL MATERIALS James Wotherspoon Fisher,

Edward William Wheatley, and Harold Bates, Spondon, near Derby, England, assignors to Cclanese Corporation of America, a corporation oi Delaware No Drawing. Application April 1, 1949, Serial No. 85,047. In Great Britain May. 5, 19,48

1 This invention relates to improvements in spinning artificial materials, and is a continuation in part of our US. application 8.1%. 784,306, filed Novemberi, 1947.

" QUJS. application 3., No. 784,306 describes the modification of poly-1.2.4-triazoles by reacting 4 Claims. '(Ci.18-54) known as cold drawing 5 Preferably this drawing' operation is carried out while heating the filaments',- for. examplebyzcontactswith ahot plate.

them with an aldehyde. This treatment has the the presence during the spinning operation-of the aldehyde very much facilitates the actual spinning process;

Formaldehyde is the preferred aldehydeas it reacts fairly readilyin the cold :and still more readily when heat is ap lied. This is ofimportance as the actual time --of contact of the filamerits or other materials-with the'precipitating bath is relatively short. Thus, for example, using.

formaldehyde we have obtained goodfilaments by spinning a 33% solution in acetic acidof a polyaminotriazole obtained according 'to' U; S.

application S. No. 609,031- filed nugust 4, 1945, by heat treatment ofl's'ebacicdihydrazide in of low lustre.

presence of hydrazine, the polymer having an in- 1 trinsic viscosity of about 0.6, into "a coagulating bath consisting of an aqueous solution of. caustic soda containing formaldehyde. The irate. of

.reaction of the formaldehyde. Thusif' both the 85." spinning should be, correlated with; the rate of- I spinning dope and the-'coagulatingjbath are at room temperature, low' spinning-"spee'dsv should be used in order to "give the formaldehyde time to react in the coagulating ibath, so th B -tQth C flIQ-Q ments on emerging from the bathghavesufiicient strength. However, by heating either. the spinning dope or th'coagulating iiath or both,vhigher spinning speeds maybe achieved. We have successfully used coagulating baths consisting of a solution of 4% caustic soda-and 4% formaldehyde in water. at room temperature, and alsocoagulating baths containingelaqfi 9f callsti fsodaand 02-05% fornialdehydeat' 'i'aised "temperatures, for example -temperatures;of 40-80 6., .either of the dope alone' or ofboth bath.

The filaments, after-formation. 1nthe above manner, may drawn out (the process-usually ll unit.

demand c a u at The filaments should non-of course; heated I to-a. temperature near the melting point of the I The following examples inven- Example 1 A spinning bath 9 feet in length, 9 inches 'wide and 6 inches deep was charged to a depth of 4 /2 inches with a coagulating bath consisting of 4% caustic soda and 4% formaldehyde in-water. A spinning jet unit consisting of stainless steel was mounted so as to extrude into the bath-and was charged with a solution of a poly'aminotriazole '-obtained according to Example 11 of British Specification No. 612,609 in 99% aqueous acetic acid, the concentration being 33% byweight. Using asinglehole spinning jet of 0.2 and extruding under a nitrogen pressure of 300 lbs. per square inch, a continuous mon'ofllwas spun at the. rate of 2-metres per minute, the monofil being collected on a banking machine. The yarn so produced had elastic-likeproper-ties land was Example 2 f I Example 1 was repeated using a multi-holeje with 0.1 mm. holes. The yarn was similar in appearance and nature to the monofil obtained according to Example 1.-

Example :3-

.1 Example 2 was repeated usingga-coagulating bath consisting of 2% caustic soda and 2% formaldehyde dissolved in water. I After spinning, the' yarn was drawn out to about 200% of its initial length while passing over -aliot plate. The-reand an extension of grams per denier I Exampie 4} .Example 2 was repeatedxusing'i;a coagulating' bath containing 1% ofcaustic soda enemasof formaldehyde in water. A ain the-yarn produced wasfvery easily cold; drawn and s howed aj tenacity at break of '1;8;,-g ramsper denier and" extension. I M

Examples J "Example 4 was repeated but in this the pinning solution was, raisedlto 8 0 C. by passin! steam through a jacket surrounding the-spinnin suiting yarn had a tenacity." awar ness-1. a

The'coaeulatingbath was maintainedat' 25 C. The extrusion rate of the yarn was 6 metres per minute. The resulting yarn showed a higher lustre than that produced in the preceding examples.

Example 6- A 30% solution of the same polymer was made up in 99% acetic acid and spun into a bath of 1% caustic soda and 0.25% formaldehyde in water, using a multi-hole jet the holes of which were 0.1 mm. in diameter. In this case the spinning solution and the bath were both maintained at 45431? C. and the spinning speed was 30 metres per minute. The resulting filaments had a soft texture and a higher lustre than those of th preceding example.

Having described our invention, what we desire to secure by Letters Patent is:

1. Process for the production of artificial filaments, bristlesand films. which comprises spinning a solution of a linear polymer containing in its structural unit the 4-amino-1.2.4-triazole ring in acetic acid into an aqueous coagulating bath containing caustic soda and formaldehyde.

2. Process for the production of filaments. bristles. films and the like, which comprises spinning a solution of a linear polymer containing in its structural unit the 4-amino-1.2.4-triazole ring in acetic acid into an aqueous bath containing caustic soda and formaldehyde each in a concentration up to 4%.

3. Process for the production of filaments, which comprises spinning a solution of a linear polymer containing in its structural unit the 4- amino-1.2.4-triazole ring in acetic acid into an aqueous bath containing caustic soda and formaldehyde each in a concentration up to 2%- 4. Process for the production of filaments, which comprises spinning a solution of a linear polymer containing in its structural unit the 4- amino-1.2.4-triazole ring in acetic acid into an aqueous bath containing caustic soda in a concentration of about 1% and formaldehyde in a concentration of 02-05%, the spinning solution and the coagulating bath being at a temperature of JAMES WOTHIERSPOON FISHER. EDWARD WILLIAM WHEATLEY.

REFERENCES CITED The following references are of record in the file of this patent:

UNITED STATES PATENTS 

1. PROCESS FOR THE PRODUCTION OF ARTIFICIAL FILAMENTS, BRISTLES AND FILMS, WHICH COMPRISES SPINNING A SOLUTION OF A LINEAR POLYMER CONTAINING IN ITS STRUCTURAL UNIT THE 4-AMINO-1.2.4-TRIAZOLE RING IN ACETIC ACID INTO AN AQUEOUS COAGULATING BATH CONTAINING CAUSTIC SODA AND FORMALDEHYDE. 